CN103604764A - Method for detecting fluorescent brightener in food and paper packaging thereof - Google Patents
Method for detecting fluorescent brightener in food and paper packaging thereof Download PDFInfo
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Abstract
The invention discloses a method for detecting a fluorescent brightener in food and paper packaging thereof. The method comprises the following steps: (1) preparing fluorescent brightener standard solutions with different concentrations; (2) preparing a standard curve between the fluorescent brightener concentration and absorbancy; (3) extracting a fluorescent brightener; and (4) arranging the filtrate in the step (3) in a quartz cuvette being 1cm, measuring the absorbancy at 350nm by adopting an ultraviolet spectrophotometer, performing a blank experiment, and calculating to obtain the content of the fluorescent brightener in the food and paper packaging thereof according to the standard curve obtained in the step (2). The fluorescent brightener detection in the food and the paper packaging thereof is realized by adopting ultraviolet spectrophotometry, the experimental apparatus is simple, the operation is convenient, and the method has the advantages of quantitative analysis, low detection limit, high repeatability and the like and is suitable for measurement of micro and trace components.
Description
Technical field
The present invention relates to the detection method of fluorescer in food and papery packing thereof.
Background technology
Fluorescer is that a class absorbs ultraviolet light, launches the fluorescent material of blueness or purplish blue coloured light.As fluorescer, its molecule all has the planar conjugate system being formed by pi-electron, and structure is as Fig. 1.The compound of this class formation absorbs after ultraviolet ray (300-400 nm), and electronics is energized into active state from ground state, gets back to again ground state at the utmost point in the short time, can emit wavelength be the fluorescence of 420-450 nm.Why fluorescer has whitening effect, and reason is that absorption has the material of fluorescer but also transfer sightless ultraviolet light to visible ray, to reflect being radiated at VISIBLE LIGHT EMISSION on object out, has increased object to reflection of light rate.Another of fluorescer brightens reason can be by complementary colors principle explanation in optics.Research discovery, the flavescence of white this tertiary colour is damaged formation the due to blue wave band light relative intensity in the light reflecting from irradiated object.Thereby early stage people use some blueness to article blueing to cover its yellowing, but cause that article brightness declines, and has visually produced dim sensation.Fluorescer sends blue or hepatic fluorescence, just in time mends that it is damaged, and has recovered the white of article.
Fluorescer is that in a kind of structure, existing phenyl has again sulfonic organic compound.It is reported, once the protein bound in fluorescer and human body is just difficult to excrete by eubolism.Meanwhile, fluorescer can greatly weaken immunity and wound healing ability, once put aside excessively in human body, except the vitals such as liver are caused serious harm, also can bring out cell carcinogenesis, is one of potential carcinogenic factor.For add fluorescer country in general paper products, there is no strict restriction, but in food wrapper and paper for daily use, forbid the existing relevant regulations of fluorescer and become social consensus, the production of articles license detailed rules for the implementation > > such as China < < paper wrapper for food, container clearly stipulate must not use fluorescer in production run.Nowadays, the testing agency of many countries and regions has classified fluorescent substance as the test item of these paper kinds.
The analytical approach of fluorescer generally has molecular fluorescence photometry, ultraviolet spectrophotometry, thin layer chromatography and high performance liquid chromatography.
Thin layer chromatography complicated operation, and can only Semi-qualitative quantitative.Fluorescence spectrophotometry utilizes the fluorescence spectrum of fluorescer to analyze, and has experiment easy, the advantage that detectability is low.Luo Guan medium [1], Pan Keliang etc. [2] report the fluorescence spectrophotometry of fluorescer respectively.The content of fluorescer in Wei-Chuan Shu etc. [3] have been used Ion-pair Liquid Chromatography methods analyst washing agent and surface water.Hsin-Chang Chen etc. [4] have been used chromatography of ions-mass Spectrometry for Determination paper handkerchief, toilet paper, the content of fluorescer in infant-wear and Environmental Water.Because liquid phase chromatography has very powerful separating power, can realize the robotization of operation, easy and simple to handle, can to fluorescer, carry out qualitative and quantitative analysis well.2000, Dong Zhongsheng etc. reported the ultraviolet spectrophotometry of measuring fluorescer CXT intensity.
Existing national standard, industry standard, provincial standard and corresponding rules have only proposed simple observational measurement requirement and detection method, without quantitative requirement and detection method.The analytical approach > > of State Standard of the People's Republic of China GB 11680-89 < < base paper for foodstuff packaging hygienic standard > >, State Standard of the People's Republic of China GB 3561-89 < < base paper for foodstuff packaging hygienic standard has all proposed to check the quilitative method of fluorescer under uviol lamp.The analytical approach > > of State Standard of the People's Republic of China GB/T 5009.78-2003 < < base paper for foodstuff packaging hygienic standard is the new standard of the analytical approach > > of GB 3561-1989 < < base paper for foodstuff packaging hygienic standard instead, for fluorescence detection method, does not change.Detection method and the above-mentioned national standard method of the fluorescer of mentioning in the detection > > of fluorescent material in the light industry standard QB 2294-2006 < < of People's Republic of China (PRC) dixie cup > >, the agricultural industry criteria NY/T 1257-2006 < < of People's Republic of China (PRC) edible fungi are basically identical.2007, State Administration for Quality Supervision and Inspection and Quarantine has printed and distributed the production of articles license detailed rules for the implementation > > such as < < paper wrapper for food, container, and detailed rules for the implementation contain 21 products of 2 class.Detailed rules and regulations all propose fluorescent substance detection for multiple product and should be qualified requirement.The promulgation of these detailed rules for the implementation, has embodied the raising that China requires for food packaging safety, has embodied the attention of China to fluorescer test item in the goods such as paper wrapper for food, container.The detection method that in the provincial standard DB51/T 907-2009 < < of Sichuan Province edible fungi, fluorescer detects the mensuration > > regulation of fluorescer in rules > >, the little flour of the provincial standard DB 13/T 1114-2009 < < of Hebei province does not have essential difference with above-mentioned state object detection method yet.
Summary of the invention
The invention provides the detection method of fluorescer in a kind of food and papery packing thereof, the fluorescer that adopts ultraviolet spectrophotometry to realize in food and papery packing thereof detects, experimental apparatus is simple, easy to operate, quick, having can quantitative test, detection limit is low, reproducible, can meet the advantages such as request for utilization, is suitable for the mensuration of trace and trace components.
The technical solution used in the present invention is:
In food and papery packing thereof, a detection method for fluorescer, comprises the steps:
(1) the fluorescer standard solution of preparation variable concentrations: accurately take 0.01g fluorescer, add alkaline solution, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution; Standard reserving solution be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to variable concentrations; The pH value of described alkaline solution is 8.5-9.5;
(2) preparation standard curve: adopt ultraviolet spectrophotometer under 350nm, the standard solution of the variable concentrations of preparation in step (1) to be detected, make the typical curve between fluorescent brightening agent concentration and absorbance;
(3) extract fluorescer; Get outturn or food samples 1.0-2.0g, shred and be placed in beaker, add 20-30mL alkaline solution, room temperature, dark place, ultrasonic extraction 20-30min, filter; The pH value of described alkaline solution is 8.5-9.5;
(4) fluorescent brightener levels is measured: the filtrate of step (3) is placed in to 1 cm quartz colorimetric utensil, adopts ultraviolet spectrophotometer to measure absorbance under 350nm, carry out blank assay simultaneously; The typical curve obtaining according to step (2) calculates the content of fluorescer in outturn or food samples.
Preferably, the standard items that step (1) Plays solution is used adopt one or more in VBL fluorescer, CXT fluorescer, 31# fluorescer, BA fluorescer and BBU fluorescer.
Preferably, alkaline solution is the aqueous solution of sodium carbonate, sodium bicarbonate or NaOH.
Preferably, in step (3), outturn is cut into 1-1.5cm
2fragment, food samples is cut into 1-1.5 cm
3fritter.
Preferably, in step (1), the concentration of fluorescer standard solution is: 5mg/ L, 10mg/ L, 20 mg/ L, 40 mg/ L, 80 mg/ L.
In food and papery packing thereof, fluorescer is VBL fluorescer, CXT fluorescer, 31# fluorescer, BA fluorescer and BBU fluorescer, above fluorescer is Stilbene-based Fluorescent Brighteners, structure and properties is similar, there is similar uv absorption, therefore the multiple fluorescer coexisting is measured and had theoretical foundation simultaneously.
The compound method of the fluorescer standard solution of variable concentrations is: accurately take 0.01g fluorescer, add the alkaline solution that pH value is 8.5-9.5, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution; Standard reserving solution be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to variable concentrations.
In outturn or food samples, the cubage method of fluorescer is: the absorbance by the filtrate of actual measurement deducts blank, then from typical curve, find the concentration of fluorescer in filtrate, the quality of the content of fluorescer in outturn or food samples=(volume of the concentration * filtrate of fluorescer in filtrate)/outturn or food samples.
The beneficial effect that adopts technique scheme to produce is:
The advantages such as the fluorescer that the present invention adopts ultraviolet spectrophotometry to realize in food and papery thereof packing detects, and experimental apparatus is simple, easy to operate, and having can quantitative test, detection limit is low, reproducible, are suitable for the mensuration of trace and trace components.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the canonical plotting between fluorescent brightening agent concentration and absorbance in embodiment 1;
Fig. 2 is the impact of pH value on extraction effect;
The impact of Fig. 3 temperature on extraction effect;
The impact on extraction effect of Fig. 4 extraction time;
The different fluorescer absorption spectrums of Fig. 5;
The impact of Fig. 6 illumination on fluorescent whitening agent VBL stability;
The impact of Fig. 7 illumination on fluorescer 31# stability;
The impact of Fig. 8 illumination on fluorescer BBU stability;
Fig. 9 pH value is on the impact of measuring.
Embodiment
In following embodiment, packaging for foodstuff is from market, and food is bought in market, and kind is asparagus, pleurotus eryngii, white jade mushroom, crab flavour mushroom, agrocybe, seafood mushroom and elegant precious mushroom etc.
(1) compound method of fluorescer standard solution is: accurately take 0.01gVBL fluorescer, add the alkaline solution that pH value is 8.5-9.5 to dissolve, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution, concentration is 100 mg/L.Storing solution accurately be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to 5mg/ L, 10mg/ L, 20 mg/ L, 40 mg/ L, 80 mg/ L.
(2) preparation standard curve: adopt ultraviolet spectrophotometer under 350nm, above-mentioned standard solution to be detected, make the canonical plotting (see figure 1) between fluorescent brightening agent concentration and absorbance;
(3) extract fluorescer; Getting bread dress pattern product 1.0g, is cut into 1-1.5cm
2fragment and be placed in beaker, add 20mL alkaline solution, room temperature, dark place, ultrasonic extraction 20min, filter;
(4) fluorescent brightener levels is measured: the filtrate of step (3) is placed in to 1 cm quartz colorimetric utensil, adopt ultraviolet spectrophotometer to measure absorbance under 350nm, deduct blank absorbance, obtain the absorbance of filtrate, the canonical plotting (see figure 1) obtaining according to step (2) obtains fluorescent brightening agent concentration in filtrate, and the content that calculates fluorescer in outturn according to fluorescent brightening agent concentration and sample quality in filtrate volume, filtrate is 0.5g/kg.
Embodiment 2
(1) compound method of fluorescer standard solution is: accurately take 0.01gCXT fluorescer, add the alkaline solution that pH value is 8.5-9.5 to dissolve, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution, concentration is 100 mg/L.Storing solution accurately be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to 5mg/ L, 10mg/ L, 20 mg/ L, 40 mg/ L, 80 mg/ L.
(2) preparation standard curve: adopt ultraviolet spectrophotometer under 350nm, above-mentioned standard solution to be detected, make the typical curve between fluorescent brightening agent concentration and absorbance;
(3) extract fluorescer; Get asparagus sample 2.0g, be cut into 1-1.5 cm
3fritter and be placed in beaker, add 30mL alkaline solution, room temperature, dark place, ultrasonic extraction 30min, filter;
(4) fluorescent brightener levels is measured: the filtrate of step (3) is placed in to 1 cm quartz colorimetric utensil, adopts ultraviolet spectrophotometer to measure absorbance under 350nm, carry out blank assay simultaneously; The content that the typical curve obtaining according to step (2) calculates fluorescer in outturn is 1.4g/kg.
Embodiment 3
(1) compound method of fluorescer standard solution is: accurately take 0.01gBBU fluorescer, add the alkaline solution that pH value is 8.5-9.5 to dissolve, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution, concentration is 100 mg/L.Storing solution accurately be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to 5mg/ L, 10mg/ L, 20 mg/ L, 40 mg/ L, 80 mg/ L.
(2) preparation standard curve: adopt ultraviolet spectrophotometer under 350nm, above-mentioned standard solution to be detected, make the typical curve between fluorescent brightening agent concentration and absorbance;
(3) extract fluorescer; Get French fries wrapping paper sample 1.5g, be cut into 1-1.5cm
2fragment and be placed in beaker, add 25mL alkaline solution, room temperature, dark place, ultrasonic extraction 25min, filter;
(4) fluorescent brightener levels is measured: the filtrate of step (3) is placed in to 1cm quartz colorimetric utensil, adopts ultraviolet spectrophotometer to measure absorbance under 350nm, carry out blank assay simultaneously; The content that the typical curve obtaining according to step (2) calculates fluorescer in outturn is 1.9g/kg.
Embodiment 4
(1) compound method of fluorescer standard solution is: accurately take BA fluorescer 0.004g and 31# fluorescer 0.006g, add the alkaline solution that pH value is 8.5-9.5 to dissolve, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution, concentration is 100 mg/L.Storing solution accurately be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to 5mg/ L, 10mg/ L, 20 mg/ L, 40 mg/ L, 80 mg/ L.
(2) preparation standard curve: adopt ultraviolet spectrophotometer under 350nm, above-mentioned standard solution to be detected, make the typical curve between fluorescent brightening agent concentration and absorbance;
(3) extract fluorescer; Get seafood mushroom sample 1.3g, be cut into 1-1.5 cm
3fritter and be placed in beaker, add 25mL alkaline solution, room temperature, dark place, ultrasonic extraction 25min, filter;
(4) fluorescent brightener levels is measured: the filtrate of step (3) is placed in to 1 cm quartz colorimetric utensil, adopts ultraviolet spectrophotometer to measure absorbance under 350nm, carry out blank assay simultaneously; The content that the typical curve obtaining according to step (2) calculates fluorescer in outturn is 2.1g/kg.
One, the optimization of extraction conditions
The selection of 1.1 alkaline solutions
?the extraction agent of fluorescer mainly contains methenyl choloride, DMF, DMA, chloroform, tetrahydrofuran, ethanol, methyl alcohol and water etc.The present invention, according to the illegal water-soluble good character of fluorescer of adding in paper grade (stock) fluorescer and food, extracts the fluorescer in sample with alkali lye, to reach reduction cost of determination, reduces the object of environmental pollution.Conventional alkaline matter is sodium carbonate, sodium bicarbonate, NaOH.In order to determine whether these three kinds of alkaline extraction agents exert an influence to the extraction of fluorescer in sample, and the sodium carbonate that is 9.0 by pH value respectively in experiment, sodium bicarbonate, sodium hydrate aqueous solution extract respectively the fluorescer in paper products.Experiment shows, alkali kind is on measuring without impact.Therefore the aqueous solution that the present invention chooses sodium carbonate, sodium bicarbonate, NaOH is as alkaline solution.
The selection of 1.2 optimal pHs
PH value is chosen as 7.0,8.0,9.0,10.0,11.0 and 12.0, and result as shown in Figure 2.In Fig. 2, data are known, when pH value is greater than 8.0, can comparatively fully extract fluorescer.Therefore the pH value of alkaline solution is made as to 8.5-9.5.
extract the selection of temperature
Under different temperatures, carry out abstraction and quantification, extract temperature and be chosen as respectively 20 ℃, 40 ℃, 60 ℃, 80 ℃.Measurement result is shown in Fig. 3.Therefore as can be seen from Figure 3, the extraction efficiency of fluorescer changes with the variation of extraction temperature hardly, and following experiment is selected and under room temperature, extracted operation.
the selection of extraction time
Extraction time is chosen as respectively 5 min, 10 min, 20 min, 30 min, 40 min, 50 min, and measurement result is shown in Fig. 4.As can be known from Fig. 4, during 20 min, the fluorescer in sample has extracted completely, and therefore, the selective extraction time is 20-30min.
the impact of leaching process on fluorescer
It is reported, fluorescer is subject to the change that affects meeting recurring structure of the factors such as illumination, and the extracting method that this problem adopts is room temperature, dark place, ultrasonic extraction.Instability based on fluorescer, this problem is carried out abstraction and quantification to the standard solution of variable concentrations, relatively through extracting the variation of operation front and back absorbance.Table 1 and table 2 are the contrast of absorbance before and after fluorescent whitening agent VBL and fluorescer BBU extract.
The impact of table 1 leaching process on fluorescent whitening agent VBL
The impact of table 2 leaching process on fluorescer BBU
As can be seen from the table, the extraction process after optimization has no significant effect the absorbance of fluorescer.(the absorbance variation before and after fluorescer CXT, fluorescer 31#, fluorescer BA extraction is similar with fluorescer BBU to fluorescent whitening agent VBL.）
2, the optimization of condition determination
In order to improve the whitening effect of fluorescer, the manufacturer of some papermaking producers or fluorescer can be used or produce compound fluorescer.Be about to 2 kinds or fluorescer of more than two kinds and mix, for a kind of fluorescer of equivalent, through the fluorescer of composite synergistic, often there is the whitening effect of observable enhancing.Because may there is more than a kind of fluorescer in paper, therefore detect multiple fluorescer has realistic meaning simultaneously very much.Chromatographic process has ability separated and that measure concurrently, detects, but need multiple fluorescer standard model need to be for various fluorescer drawing curves in the time of can be for multiple fluorescer, and testing cost is high, and workload is larger.Because spectrophotometric method can not make the various ingredients in sample separated in mensuration process, so some analytical work persons have explored the problem that spectrophotometric method is measured the similar mensuration thing of multiple character simultaneously.The artificial fluorescer adding is Stilbene-based Fluorescent Brighteners in paper products and in food, and structure and properties is similar, has similar uv absorption, therefore the multiple fluorescer coexisting is measured and is had theoretical foundation simultaneously.
the selection of maximum absorption wavelength
The absorption spectrum of fluorescent whitening agent VBL, fluorescer CXT, fluorescer 31#, fluorescer BA and fluorescer BBU is as Fig. 5.In Fig. 5, show, these fluorescer maximum absorption wavelengths are respectively 347 nm, 355 nm, 347 nm, 351 nm and 355 nm.Come from the similarity of 5 kinds of fluorescer structures, its maximum absorption wavelength is close, and therefore selecting 350 nm is lambda1-wavelength.
the comparison of molar absorptivity
Take fluorescent whitening agent VBL, fluorescer CXT, fluorescer 31#, fluorescer BA and fluorescer BBU separately the standard solution of variable concentrations be determination object, measure absorbance drawing curve.The molar absorptivity of the various fluorescers that calculated by working curve is listed in table 3.As can be known from the table data, the molar absorptivity of 5 kinds of fluorescers is basically identical, can measure simultaneously.The similarity of fluorescer absorptivity comes from the similarity of its structure.
The molar absorptivity of table 3 fluorescer
2.3 absorbance additive properties are investigated
Get fluorescer mixed standard solution and measure absorbances at 350 nm, and the absorbance sum of measuring during with various fluorescer individualism compares.The additive properties experimental result of composite fluorescence whitening agent is as table 4-7.From experimental result, the calculated value of total absorbance and measured value difference are less, measure total amount feasible simultaneously.During fluorescer compound use, how by 2 kinds of fluorescer compound uses, 3 kinds above rare, so the additive property of absorbance is investigated when this problem only coexists to 2 kinds and 3 kinds of fluorescers.The combination variety of composite fluorescence whitening agent is more, and data are not listed one by one.
Table 4 fluorescent whitening agent VBL and fluorescer CXT additive property are investigated
Table 5 fluorescer BA and fluorescer 31# additive property are investigated
Table 6 fluorescent whitening agent VBL and fluorescer BBU additive property are investigated
Table 7 fluorescent whitening agent VBL, fluorescer 31# and fluorescer BBU additive property are investigated
2.4 study on the stability
This partial content is discussed on the impact of fluorescer stability on illumination, pH value.
the impact of illumination
The optical brightener solutions of 1 mg/L is placed in to (available light) and dark place placement in laboratory, investigates the stability of fluorescer.Fig. 6-8 are respectively fluorescent whitening agent VBL, fluorescer 31# and fluorescer BBU absorbance-time curve under different light rays, the absorbance of fluorescer XCT and fluorescer BA is consistent with time curve and above-mentioned curved line relation, repeats no more.From Fig. 6-8, can find out the stability of fluorescer good stability in the dark under indoor natural light.Under Indoor Natural light, in 60 min, significantly do not change, 30 min internal stabilities are better.For general spectrophotometry, in 30 min, can complete mensuration work, so the stability of fluorescer under indoor light can meet the requirement of spectrophotometry.
PH value
impact
Paper grade (stock) and the fluorescer that is illegally added into the Stilbene-based in food are anionic dye, different solubility in the solution of different pH values.Fig. 9 has represented under different pH values, is the absorbance of fluorescent whitening agent VBL, fluorescer CXT, fluorescer 31#, fluorescer BA and the fluorescer BBU of 20 mg/L for concentration.As seen from Figure 9, when pH value is 4 and 5, the absorbance of fluorescent whitening agent VBL, fluorescer CXT, fluorescer 31#, fluorescer BA is on the low side, the reason that produces this situation is mainly because hydrophilic radical sulfonic group compares less in the molecular structure of 2S type fluorescer, only have two, thus water-soluble relatively poor, when pH value is lower, fluorescent brightening agent molecule is assembled, and solution no longer meets law of light absorption (youth uncle one law of Beer).When pH is 6-12, the absorbance of these 4 kinds of 2S type kind fluorescers is stable.In molecular structure for 4S type fluorescer BBU, have 4 sulfonic groups, good water solubility is in 2S type fluorescer, so fluorescer BBU all has more stable absorbance when pH value 4-12.The structure of considering fluorescer is held impact that point, variation of ambient temperature may bring and the unification of operating conditions, and the pH value of detected solution is elected 8.5-9.5 as.Because the pH value of fluorescer extraction agent is 8.5-9.5, so after extracting, do not adjust pH value and directly measure.
, leaf of bamboo paper is on the impact of measuring
Bamboo is one of raw material of papermaking, and bamboo has natural fluorescence.In order to study, take bamboo pulp as raw material.In order to study, to take natural fluoresence composition in the paper that bamboo pulp is raw material and whether to measuring, have interference, this problem is observed under uviol lamp 2 kinds of dry leaf of bamboves, there is no fluorescence phenomenon, these 2 kinds of dry leaf of bamboves have been carried out to extraction and the measurement operation as described in 3.2, result shows, extract solution of bamboo leaves does not absorb at 350 nm.Its reason may be destroyed in dry process for the chlorophyll in the leaf of bamboo, no longer has photoluminescent property.
, detectability, precision and the recovery mensuration
To edible fungi sample, used for packing foods pattern product with and mark add sample and measure, result is as shown in table 8 and table 9.In edible fungi, do not detect fluorescer, in Partial Food wrappage, detect fluorescer.When mark adds concentration and is 0.2 g/kg, 1.0g/kg and 3.0g/kg, the recovery is 95.6%-108%, and standard deviation is 2.1%-4.3% (n=3).The range of linearity is 0.1-3 g/kg, at this scope internal linear correlativity R
2=0.9992; Method detects and is limited to 0.03 g/kg, is quantitatively limited to 0.1 g/kg.
The measurement result of fluorescer in table 8 edible fungi
The measurement result of fluorescer in table 9 packaging for foodstuff paper using
Claims (5)
1. a detection method for fluorescer in food and papery packing thereof, is characterized in that comprising the steps:
(1) the fluorescer standard solution of preparation variable concentrations: accurately take 0.01g fluorescer, add alkaline solution, be stirred to whole dissolvings, proceed to constant volume in 100 mL volumetric flasks, obtain fluorescer standard reserving solution; Standard reserving solution be take to the alkaline solution that pH value is 8.5-9.5 and be diluted to variable concentrations; The pH value of described alkaline solution is 8.5-9.5;
(2) preparation standard curve: adopt ultraviolet spectrophotometer under 350nm, the standard solution of the variable concentrations of preparation in step (1) to be detected, make the typical curve between fluorescent brightening agent concentration and absorbance;
(3) extract fluorescer; Get outturn or food samples 1.0-2.0g, shred and be placed in beaker, add 20-30mL alkaline solution, room temperature, dark place, ultrasonic extraction 20-30min, filter; The pH value of described alkaline solution is 8.5-9.5;
(4) fluorescent brightener levels is measured: the filtrate of step (3) is placed in to 1 cm quartz colorimetric utensil, adopts ultraviolet spectrophotometer to measure absorbance under 350nm, carry out blank assay simultaneously; The typical curve obtaining according to step (2) calculates the content of fluorescer in outturn or food samples.
2. the detection method of fluorescer in food according to claim 1 and papery packing thereof, is characterized in that the standard items that described step (1) Plays solution is used adopt one or more in VBL fluorescer, CXT fluorescer, 31# fluorescer, BA fluorescer and BBU fluorescer.
3. the detection method of fluorescer in food according to claim 1 and papery packing thereof, is characterized in that described alkaline solution is the aqueous solution of sodium carbonate, sodium bicarbonate or NaOH.
4. the detection method of fluorescer in food according to claim 1 and papery packing thereof, is characterized in that, in step (3), outturn is cut into 1-1.5cm
2fragment, food samples is cut into 1-1.5 cm
3fritter.
5. according to the detection method of fluorescer in the food described in claim 1,2,3 or 4 and papery packing thereof, it is characterized in that the concentration of fluorescer standard solution in step (1) is: 5mg/ L, 10mg/ L, 20 mg/ L, 40 mg/ L, 80 mg/ L.
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| CN105628823A (en) * | 2016-02-04 | 2016-06-01 | 中山出入境检验检疫局检验检疫技术中心 | Method adopting high performance liquid chromatography to detect fluorescent whitener in flour |
| CN105628823B (en) * | 2016-02-04 | 2017-07-04 | 中山出入境检验检疫局检验检疫技术中心 | A kind of method of fluorescent whitening agent in use high performance liquid chromatography detection flour |
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| CN107084936A (en) * | 2017-04-24 | 2017-08-22 | 沃奇中 | The assay method of transportable property fluorescent whitening agent in toilet paper |
| CN108166243A (en) * | 2017-12-07 | 2018-06-15 | 桐乡市东企纤维整理有限公司 | A kind of acrylic fibers staple in bulk unstressed configuration whitening process |
| CN111458304A (en) * | 2020-04-10 | 2020-07-28 | 海信（山东）冰箱有限公司 | Fluorescent whitening agent detection system of washing machine |
| CN111458304B (en) * | 2020-04-10 | 2023-04-18 | 海信冰箱有限公司 | Fluorescent whitening agent detection system of washing machine |
| CN113376272A (en) * | 2021-05-28 | 2021-09-10 | 江苏天成纸业有限公司 | Efficient detection method capable of detecting multiple fluorescent whitening agents in paper product |
| CN113834794A (en) * | 2021-09-29 | 2021-12-24 | 浙江宏达化学制品有限公司 | Detection method for rapidly detecting quality of fluorescent whitening agent |
| CN114034529A (en) * | 2021-11-11 | 2022-02-11 | 广东睿鹏材料科学有限公司 | Detection pretreatment method of anti-counterfeiting material containing trace fluorescent groups |
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